Installation for treatment of textile materials

ABSTRACT

Apparatus for the treatment of textile materials in a bath, such as a dyeing bath containing solvents and diluents for the dye, including an enclosure for the dyeing, means for continuously drawing off a fraction of the bath, means for separating the bath components, recycling means for reintroducing the separated portion into the bath, and regulating devices for regulating the volume of the fraction drawn off from the enclosure.

' United States Patent I 1 Field of Search .;...-..6 s/1s R,: 18 F, 18 c, 13 R CONDENSER EXTR ACTOR V Blane et al. Jan. 16, 1973 [54] INSTALLATION FOR TREATMENT OF [56] References Cited TEXTILE MATERIALS UNITED STATES PATENTS [75] Inventors: Remy Blane, Lyon; Alain Chapuis,

s c 'euRhone; Pierre Gagne 3,177,126 4/1965 Charrean ..68/l8 C X I Villeurbanne, all of France Primary Examiner william I. Price [73] Assignee Soltex, Paris, France Att0mey-Browdy & Neimark [22] Filed: 3 May 6, 1971 57 ABSTRACT [21] Appl. NO-I 14 ,836 Apparatus for the treatment of textile materials in a I bath, such as a dyeing bath containing solvents and [30] Foreign Application Priority Data diluents for the dye, including an enclosure for the I dyeing, means for continuously drawing off a fraction May 15,19,7 0 I -Firance .r ..70l774l of the bath, means for Separating the bath ponents, recycling means for reintroducing the C llseparated portion into the bath and regulating devices for regulating volume of the fraction drawn Off from the enclosure.

11 Claims, 2 Drawing Figures summon coLuuu DYEING ENCLOSURE PATENTEDJAN 16 I973 SHEET 2 OF 2 FIG. 2

//V VE/V TORS REMY BLANC ALAIN CHAPUIS PIERRE GAGNE 6% W1 HMML A T TORNEYS INSTALLATION FOR TREATMENT OF TEXTILE MATERIALS I The present invention relates to a novel installation for discontinuously treating textile fibers and materials in a bath containing several vehicles of the treating agent, which permits the removal, duringthe operation and in a regulated way, at least one of the vehicles. This apparatus is, for example, usable in the s-called exhaustion dyeing.

There are already various types of installations adapted for the treatment or dyeing of textile materials in an anhydrous or aqueous medium. But the various techniques described until now, which relate to installations for continuous dyeing as well as for discontinuous dyeing, are for the most part, specific to the textile materials to be dyed and to the recovery and regeneration of the solvents used. Thus, for example, a dyeing technology is described in U. S. appln. Ser. No. 58,973, Hess et al., filed July 28, 1970 which is a combination of means some of which are known, while others, taken separately, are novel and which includes a padding in which the textile material is impregnated continuously with a mixture of solvents in which is dissolved the convenient dyestuff(s), and a series of enclosures at such temperatures that one of the constituents of the solvent mixture is vaporized alone, the textilev material thereafter being submitted to the vapor of another sol- The novel apparatus according to the present invention may be used to achieve the hereinabove dyeing process. However it should be noted that the apparatus can be used in any process of treating textiles in a bath containing. as vehicles of the treating agent, at least two components which can be separated and from which at least one is to be removed during the treatment.

In its most general form, the new installation according to the present invention comprises:

an enclosure for treating textile materials in a bath,

meansfor drawing off continuously a fraction of the bath,

means for separating the bath components to be removed from the fraction,

a recycling circuit ensuring re-introduction into the treatment enclosure, of the liquid portion obtained after separating the bath components, and

regulating devices, permitting the regulation of the volume of the fraction drawn off from the enclosure. I Optionally the quantity of component to be removed may also be regulated. The treatment enclosure may be any device commonly used in such treatments. For example, in the case of dyeing, a vat may be used which is of a known type provided with cooling and heating elements necesvent in which the dyestuff is insoluble, and finally this l'ast solvent is removed by evaporation. This technology of continuous dyeing, suitable only for textiles in fleece form, such as fabrics, jerseys, etc; needs phases of successive recovering of the various solvents used. 7

ln a generalway, when dyeing is achieved in a continuous way, the recovery of the various constituents of the bath is easily achieved by the utilization of several evaporation enclosures placed in series of a treatment chain. But when dyeing is conducted in a discontinuous manner by exhaustion and needs a long period of contact of the textile material with the bath containing the coloring agent, the recovering of one or several bath constituents cannot be done during the dyeing .opera-.

tion, but only after the end of the dyeing operation.

There has now been found a new installation, which under the most favorable conditions of temperature and pressure yields excellent results for treating textile materials which may be in various forms and to remove from the bath, while the treatment is being conducted one or several of its components, in order thatthis removal can be completed at the latest,-at the end of the operation. I

ln U. S. Appln. Ser. No. 33.094 filed Apr. 29, 1970 by Blane et al., there is described a dyeing process by I the exhausting method, in a bath containing at least onepolar organic solvent in which the dyestuffsare soluble and one non-polar solvent in which the dyestuffs are'in soluble or only slightly soluble and according to which bath. When it is removed in the liquid phase it may further comprise or have one or more of the following devices: a thermal exchanger in order to modify, if necessary, the temperature of this fraction of the bath, a pump allowing the drawing off of this fraction of the bath, the flow rate of which may be constant or variable with regard to time, aregulat ing device for the rate of drawn off fraction, and, especially for the case in which the pressure in the enclosure is super-atmospheric, and a valve to expand the liquid mixture. When it is operated in the vapor phase, this means may also be fitted' with a thermal exchanger; they comprise generally a regulating device for the rate of drawn oft fraction.

The means for separating the bath components may be chosen among all devices of known type which are based upon the different volatilities of the mixture components. These devices are useful because, in most cases, the drawn off fraction, even if in vapor phase,

' contains at least a low proportion of the component the polar solvents may be- .progressively removed from' the bath by drawing off a part of the bathin the liquid the bath in order to compensate for the drawn off part.

which is not to be removed. Thus, the latter is recovered and later recycled into the bath. Further, it is optionally possible, by this means, to recycle into the bath a part of the bath component which is to be removed. In the cases of easy separations, a flash-pot can be used, with or without a reflux system which leads to a separation of the bath components in a gaseous and a liquid phase. A distillation column can be used which is provided with a rectification section or an exhausting section or both. in every case,'at the head of the flash-pot or the column is located the extraction device for the components to be removed which comprises a piping for collecting the vapors and conducting to a condenser. Beyond the condenser there is a collecting device which, in the case of using a flash-pot with reflux or a separation column is connected to a regulating device which controls the quantity of removed component. Thus the reflux rate which depends on the quantity of removed component is regulated, which controls also the extraction speed of the component to be removed from the bath. So, the fraction drawn off from the bath undergoes a selective and controlled separation, the liquid part intended for being reintroduced in the enclosure having a perfectly controlled composition and containing optionally a determined quantity of component to be removed, this quantity being minimal at the end of the treatment of textiles. At the foot of the column or the flash-pot is the recovery system for the liquid portion, freed of all or part of the component to be removed. This system comprises generally a tank and is optionally provided with a broiler. The tank may play the part of a compensating tank if the treatment in the enclosure is achieved with a constant volume of bath.

The recycling circuit consists ofa set of piping, pump and reheaters which allows the reintroduction into the enclosure, at convenient temperature and pressure, of the liquid part remaining after separation of the component to be removed. Besides, this circuit may have a return in the enclosure located at the foot of the column, ensuring a closed circulation of the recovered component when the bath is at a maximal level.

Finally, the regulating devices play important parts in the running of the installation according to the invention. In addition to the devices which allow the control of the rate of bath fraction to be drawn off as well as the control of the rate of component to be removed which were described hereinabovethe installation according to the invention may comprise also classical regulating devices such as, for example, those which allow the control of the temperature and volume of bath in the enclosure, and so on.

The invention will be understood better by a detailed description of the parts and operation of the installations represented in FIGS. 1 and 2 wherein:

FIG. 1 represents a scheme of the whole of the characteristic parts of the new installation for dyeing operations wherein the bath fraction is drawn off in the liquid phase.

FIG. 2 represents a variant of the general scheme of the drawing off of the fraction, a thermal exchanger 8 and a valve 9 allows for drawing off a fraction of the dyeing bath, possibly re-heating at 8 and expanding at 9. Optionally devices 5, 6, 7 and 9 may be replaced by a pump which allows the drawing off of a liquid portion at a regulated rate. The pipe 4 leads to separation column 10, possibly provided with a rectification section 11 and an exhausting section 12. At the foot of the column is situated a tank 13 filled with diluent by means of piping l4 and used as a compensating tank for dyeing bath 2. Tank 13, possibly provided with a boiler 15, recovers the liquid fraction arriving at the foot of the column. On the bottom of tank 13 is located a pipe 16 connected to a pump 17 and a thermal exchanger 18. Upstream of the thermal exchanger 18 a return pipe 19 connects with a tank 13. A valve 20 is provided in pipe 19 driven by regulator 21 mounted on levelthrottles 22 and 23 of dyeing enclosure. At the head of the column 10 is located a pipe 24 which connects with a condenser 25, connected to tank 26. The bottom of tank 26 is provided with a piping 27, of siphon type, opening at the column head 10, and also with a piping 28 provided with an extractor 29 having a constant volume, such as a dosimeter-pump or valve, driven by drawing off regulator 30.

In the arrangement shown in FIG. 2 in which the drawing off is in the vapor phase, piping 4 located at the upper portion of vat 1, is provided with the'thermal exchanger 8 and a valve 9 for regulating the rate of the drawn off fraction. v

The installation according to FIG. 2 is advantageously used when the bath fraction, drawn off in the vapor phase, contains some quantity of diluent which is to be separated and recycled.

Installation operation will be understood better by a description of the fluid circulation motion, referred to the dyeing operations.

The dyeing bath consists of a mixture of a solvent 8,, generally in minor quantity, having a boiling temperature, 1,, and with a diluent S having a boiling temperature 1 which is in most cases greater than 1,. The dyestuffs used are soluble at any temperature in S, and insoluble or relatively insoluble in S The bath is gradually heated to the required temperature. After a given time, the drawing off of a bath fraction begins.

FIG. 1 for dyeing operations wherein the bath fraction is drawn off in the vapor phase.

In order to make the description clear it will be referred in the description, as examples, to dyeing operations. The component to be removed will be called the solvent whereas the component which remains in or returns to the bath will be called the diluent.

According to FIG. 1, the dyeing enclosure 1, which may be provided with a condenser (not represented on the drawing) which contains textile material, is filled with a dyeing bath 2. Bath temperature is regulated by thermal regulator 3. A pipe 4 on which is mounted a regulating device having a diaphragm 5 for flow rate measure, a regulation valve 6 and a rate driving 7 for The withdrawn fraction flows through piping 4, is optionally reheated in 8 and expanded in 9, then is introduced into the separation column 10. After the solvent S, is condensed in 25 and stored in tank 26, the solvent is partly removed by the constant volume extractor 29, driven by regulator 30, while the remaining part is re-introduced by pipe 27 into column 10. If the pipe 27 is closed off the whole of solvent S, is stored in 26. The liquid fraction freed of or weak in S, is recovered in tank 13 and recycled at convenient temperature and pressure into the dyeing enclosure thru piping 16, pump 17, and thermal exchanger 18. If the dyeing bath volume is temporarily at its maximal level, the liquid fraction recycles into tank 13 through piping 19 and valve 20 driven by level regulator 21. Progressively the solvent S, content of the dye bath is reduced during the dyeing operation, the content of the bath in S, being very weak or non-existent at the end of the operation.

The operation of the installation according to the present invention is not exclusively limited to the use of two solvents. Solvent S, may be replaced by a mixture gives excellent results, with textile materials which are in various forms such as especially bobbins, conical bobbins, tubes, cakes, yarns, fabrics, non woven fleeces, jerseys, panels, carpets, etc.

The characteristics and advantages of the installation I according to the invention will be better understood by reference to the following illustrative non-limitating examples. I

EXAMPLE 1 The dyeing of tufted carpet composed'of polyamide 6,6 knop woolsfon jute canvas, having a total weight of l020 gr/m woundon perforated beam was conducted.

Bath composition expressed'in volumes, was as follows:

methanol 100 parts perchlorethylene 899 parts glacial acetic acid 1 part The solvent of the'dyestuffs was methanol. The dilution liquid was perchlorethylene.

The quantities of dyestuffs free from blending were, expressed in weight with regard to carpet polyamide weight (about 700 gr/m2);

C.l. Acid red 57 1.2%

C.l. Acid red 61 =0.7%

The dyeing enclosure was an horizontal autoclave, with bath circulation by means of'a pump, only in the centrifugal direction. Pressure was 3 bars while textile material/bath ratio was 1 /8 in volume.

The components separation device wasa simple flashpot including a reheater 8" and drawing off and recycling means such as they have been described previously. v

Dyeing was begun at 20C., then thebath was heated gradually. Bath admissioninto the separation device began at 70C. according to a regulated rate on the EXAMPLE 2 The dyeing of polyamide 6.6 jersey panels, having a weight of 100 g/m2 in a horizontal drum machine,

which ensured panel stirringin dyeing bath was conducted.

The bath composition, expressed in volume was as follows:

Methanol 100 parts lsopropanol 10 parts Monochlorobenzene 889 parts Glacial acetic acid: 1 part 7 the Dyestuff solvent was mixture methanol/isopropanol, while the diluent was monochlorobenzene.

The-quantities of dyestuffs free from blending, were expressed in weight with regard to polyamide jersey weight:

CI. Acid red 57: l

C.l. Acid yellow 61 0.5

The dyeing enclosure operated at atmospheric pressure, while the textile material-bath ratio was H20 in volume.

A separation column provided only with a rectification section was utilized; the apparatus included means of drawing off and recycling, such as have been described previously.

Dyeing was begun at 20C., then the bath was progressively heated up to 65C. At this temperature bath boiling began,temperature increase of the bath basis of average curve of dyestuffs ascent on polyamide 6.6 with regard to temperature.

Temperatures being those of the dyeing bath, solvent was achieved according to the removing speed of the solvents.

The percentage of removed solvents was as follows:

from 65 to C. 18% in 10 minutes from 75 to C. 57% in 18 minutes 1 from 85 to l0OC. 25% in 10 minutes After the dyeing bath was practically freed of. solvents, it was maintained at the temperature of C. for 15 minutes. i

.A rinsing was conducted, after dyeing, with monochlorobenzene at a temperature of 20C.

EXAMPLE 3 The dyeing of pure wool in bobbins of 1 kg. each, on perforated tubes placed on a material-bearer was con-- ducted.

, Bath composition by volume:

' Methanol: l03.5 parts lsopropanol 25.3 parts Perchlorethylene 870 parts Glacial acetic acid 1.2part The dyestuff solvent wasthe rnixturemethanol/lsopropanol whereas the diluent was perchlorethylene.

Dyestuffs, by weight, with respect to the to tal weight I for drawing off and recycling, such as have been described previously.

Dyeing was begun at 20C. and the bath was gradually heated. Drawing off, begun at 67, has been regulated according to the following rate, expressed in EXAMPLE 4 Wool panels, having a weight of 140 g/m2 were dyed,

in a paddle machine ensuring bath stirring and operat- V ing at atmospheric pressure, and in textile bath ratio of 1/30.

Bath composition in volumes was as follows:

Methanol: 104 parts lsopropanol 25 parts Perchlorethylene 870 parts Glacial acetic acid 1 part Dyestuffs by weight with regard to the total weight of panels:

C.l. Acid red 57 1.2

C. 1. Acid blue l29= l Separation column was provided with a rectification section; the apparatus had a means of drawing off and recycling.

The dyeing cycle was identical to that of Example 2. Solvent removal, began at 65C.. and was regulated as follows:

from 65 to 75C. 16 in 10 minutes from 75 to 82C. 43 in 18 minutes from 82 to 92C. 26 in 10 minutes from 92 to l02C.= l in minutes Dyestuff exhaustion by wool panels was practically complete, at solvent removing end.

When the term vehiclesis used herein and in the claims, it is meant to include all liquidswhich constitute the treating bath and which may be solvents for the treating agent, liquids in which the treating agent is dispersed, as well as diluents for the treating agent solution.

It will be obvious to those skilled in the art that various changes may be made without departing from the scope of the invention and the invention .is not to be considered limited to what is shown in the drawings and described in the specification.

What is claimed is: 1. Apparatus for the treatment of textile materials, in a bath containing as vehicles of the treating agent, at least two fluid components of different volatilities which can be separated, from which at least one is to be removed during said treatment which comprises:

an enclosure for treating textile materials, means for drawing off continuously a fraction of said bath, 7 means based upon the differential volatilities of the fluid bath components for separating the fluid bath components to be removed from said fraction, a recycling circuit ensuring re-introduction, into the treatment enclosure, of the liquid part obtained after separat ing bath com onents, regulating devices for regu atmg the volume of the fraction drawn off from said enclosure.

2. Apparatus according to claim 1 wherein the means i 4. Apparatus according to claim 2 wherein the means for drawing off said fraction further comprises a pump.

5. Apparatus according to claim 2 wherein the means for drawing off said fraction further comprises a regulating device for controlling the rate of drawn off fraction.

6. Apparatus according to claim 2 wherein said fluid components are both liquids and wherein the means for drawing off said fraction further comprises a valve to expand the liquid mixture.

7. Apparatus according to claim 1 wherein the means forseparating the components to be removed comprises a flashpot at the head of which is situated an extraction device for the component to be removed.

8. Apparatus according to claim 7 wherein the flashpot has a reflux system.

9. Apparatus according to claim 1 wherein the means for separating the components to be removed comprises a distillation column provided with a rectification section, at the head of which is situated an extraction device for the component to be removed.

10. Apparatus according to claim 1 wherein the means for'separating the components to be removed comprises a distillation column provided with an exhausting section, at the head of which is situated an extraction device for the component to be removed.

11. Apparatus according to claim 10 wherein the column is further provided with a rectification section. 

1. Apparatus for the treatment of textile materials, in a bath containing as vehicles of the treating agent, at least two fluid components of different volatilities which can be separated, from which at least one is to be removed during said treatment which comprises: an enclosure for treating textile materials, means for drawing off continuously a fraction of said bath, means based upon the differential volatilities of the fluid bath components for separating the fluid bath components to be removed from said fraction, a recycling circuit ensuring re-introduction, into the treatment enclosure, of the liquid part obtained after separating bath components, regulating devices for regulating the volume of the fraction drawn off from said enclosure.
 2. Apparatus according to claim 1 wherein the means for drawing off said fraction comprises a pipe.
 3. Apparatus according to claim 2 wherein the means for drawing off said fraction comprises further a thermal exchanger.
 4. Apparatus according to claim 2 wherein the means for drawing off said fraction further comprises a pump.
 5. Apparatus according to claim 2 wherein the means for drawing off said fraction further comprises a regulating device for controlling the rate of drawn off fraction.
 6. Apparatus according to claim 2 wherein said fluid components are both liquids and wherein the means for drawing off said fraction further comprises a valve to expand the liquid mixture.
 7. Apparatus according to claim 1 wherein the means for separating the components to be removed comprises a flashpot at the head of which is situated an extraction device for the component to be removed.
 8. Apparatus according to claim 7 wherein the flashpot has a reflux system.
 9. Apparatus according to claim 1 wherein the means for separating the components to be removed comprises a distillation column provided with a rectification section, at the head of which is situated an extraction device for the component to be removed.
 10. Apparatus according to claim 1 wherein the means for separating the components to be removed comprises a distillation column provided with an exhausting section, at the head of which is situated an extraction device for the component to be removed.
 11. Apparatus according to claim 10 wherein the column is further provided with a rectification section. 